EP2310781A2 - Vorrichtung zur serienmässigen gefriertrocknung - Google Patents
Vorrichtung zur serienmässigen gefriertrocknungInfo
- Publication number
- EP2310781A2 EP2310781A2 EP09765597A EP09765597A EP2310781A2 EP 2310781 A2 EP2310781 A2 EP 2310781A2 EP 09765597 A EP09765597 A EP 09765597A EP 09765597 A EP09765597 A EP 09765597A EP 2310781 A2 EP2310781 A2 EP 2310781A2
- Authority
- EP
- European Patent Office
- Prior art keywords
- camera
- freeze
- drying
- images
- evaluation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000004108 freeze drying Methods 0.000 title claims abstract description 95
- 239000003186 pharmaceutical solution Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims description 104
- 238000011156 evaluation Methods 0.000 claims description 41
- 238000005286 illumination Methods 0.000 claims description 7
- 238000001228 spectrum Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 3
- 238000012792 lyophilization process Methods 0.000 abstract 1
- 239000000126 substance Substances 0.000 description 27
- 238000012360 testing method Methods 0.000 description 14
- 230000001276 controlling effect Effects 0.000 description 11
- 238000001035 drying Methods 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 4
- 230000001419 dependent effect Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000004886 process control Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 235000013372 meat Nutrition 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000013064 process characterization Methods 0.000 description 2
- 230000001960 triggered effect Effects 0.000 description 2
- 208000031872 Body Remains Diseases 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 230000006735 deficit Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 230000036512 infertility Effects 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 235000013622 meat product Nutrition 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000010943 off-gassing Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03B—APPARATUS OR ARRANGEMENTS FOR TAKING PHOTOGRAPHS OR FOR PROJECTING OR VIEWING THEM; APPARATUS OR ARRANGEMENTS EMPLOYING ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ACCESSORIES THEREFOR
- G03B15/00—Special procedures for taking photographs; Apparatus therefor
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B5/00—Drying solid materials or objects by processes not involving the application of heat
- F26B5/04—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum
- F26B5/06—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum the process involving freezing
Definitions
- the invention relates to a device for the standard freeze-drying of pharmaceutical solutions in medical hollow bodies according to the preamble of claim 1.
- the invention further relates to a method for controlling and / or controlling the standard freeze-drying of pharmaceutical solutions in medical hollow bodies having the features of the preamble of claim 18.
- Such process parameters are, for example, the product temperature, or the temperature of the shelves of the freeze-drying apparatus, the pressure prevailing in the freeze dryer, the humidity of the atmosphere within the freeze dryer, as well as the timing of these parameters throughout the process and not least the total duration of the process .
- the values to be set in each case depend on the specific substance intended for freeze-drying. If, therefore, a freeze-drying cycle is to be developed for a substance with no previous experience in freeze-drying, the relevant parameters must be determined experimentally.
- miniaturized freeze-drying devices can be provided, which can be arranged on the sample table of a microscope.
- the course of freeze-drying is either with the naked eye or with the help of a camera through the optics of the microscope and a translucent wall of the miniaturized freeze-drying device observable.
- it can be determined, preferably in several test series, at which process parameters a cake of the frozen meat rock collapses and in which a successful process takes place.
- the process parameters determined in this way can then be transferred to the standard freeze-drying, particularly in the form of preferably limiting parameters, taking into account a safety margin, whereby the temperature sensors already described above are again used for characterizing and controlling the process.
- the object of the invention is therefore to provide a device which is capable of observing, characterizing, controlling and / or controlling the freeze-drying cycle without being able to come into direct contact with the freeze-dried product. to influence the process in an undesirable way.
- online control and / or regulation of the process parameters should be possible based on criteria that can be evaluated during the freeze-drying cycle, so that it is not necessary to resort to limit parameters previously determined in separate, independent experiments and the process parameters are always kept within an optimal range can.
- the object underlying the invention is achieved by a device having the features of claim 1.
- the device has a freeze-drying device and at least one camera, wherein images of at least one pharmaceutical solution intended for freeze-drying can be received by the at least one camera. It is characterized by the fact that the images can be used to control and / or control the freeze-drying process.
- the images recorded by the camera are therefore not used primarily to be able to subsequently attribute the success or failure of the process to a choice of specific process parameters, but instead are used to actively control and / or control the course of the process.
- images of the substance intended for freeze-drying can be taken up, which can be judged on the question of whether a collapse of the freeze-dried product is imminent or how the product develops in the course of the process.
- a test person can monitor the images on a monitor and, if necessary, intervene in the process in a regulating or controlling manner.
- the test person can determine the process parameters such as pressure, temperature, humidity in the freeze-dryer atmosphere, the times and durations of the individual phases vary directly during freeze-drying and adapt to the insights gained from the images. It is therefore possible to carry out an online monitoring of the freeze-drying. As a result, the process parameters can be moved closer to the physical limit defined by the product properties.
- a maximum possible product temperature can be selected in which the drying time is significantly shorter than in the case of the temperature selected in conventional devices, determined by a safety margin.
- the state of the frozen meat stock which can be determined from the images of the substance intended for freeze-drying, is used as a criterion for the process control, so that it is possible without prior knowledge of experimental limit parameters to drive the process close to the limit of the physically possible during its entire duration.
- the drying process is significantly more economical, because per unit of time a larger amount of substance can be freeze-dried, and because previous expensive tests for the determination of limiting parameters can be omitted. At the same time, the risk of product impairment is minimized.
- a device is also preferred which is characterized in that an evaluation device is provided which evaluates the images.
- an evaluation device may be provided which, for example, by means of an image evaluation program of the monitored and evaluated at least one camera delivered images.
- a device is also preferred in which the evaluation device serves to change parameters of the freeze-drying process.
- the evaluation device undertakes, for example by means of an image evaluation program, an evaluation of the images supplied by the at least one camera and thus assesses whether possibly parameters of the drying process have to be varied in order to ensure the desired product quality. If this is the case, the evaluation device can initiate a corresponding change in the process parameters so that they again lie within a range of values that guarantees the desired product quality.
- a device in which, on the basis of the evaluation of the images, signals can be sent from the evaluation device to a control device of the freeze-drying device and in which the parameters of the freeze-drying process can be changed on the basis of these signals.
- a control device is also provided which controls the freeze-drying device or the freeze-drying process.
- the evaluation device evaluates the images of the substance intended for lyophilization supplied by the at least one camera and in particular carries out an evaluation of the images.
- signals can be sent from the evaluation device to the control device which lead to a change in the parameters of the freeze-drying process. This is to ensure that the process parameters are always in a range of values that ensures a desired product quality.
- the object of the invention is also to provide a method which allows control and / or control of the standard freeze-drying of pharmaceutical solutions in medical hollow bodies, without causing a direct contact with the substances intended for freeze-drying or that the process in the context of the method is undesirably influenced.
- the method should enable on-line control and / or control or regulation of the freeze-drying process, whereby the process can always be kept close to the limit of the physically possible. With the aid of criteria that can be evaluated during the freeze-drying process, it should be possible to control or regulate the process parameters without having to fall back on limit parameters previously determined in extensive test series while maintaining a safety margin.
- a freeze-drying device and at least one camera and the at least one camera takes pictures of at least one intended for freeze-drying pharmaceutical Solution.
- the method is characterized in that these images are used to control and / or control the freeze-drying process. This can be done, for example, by a test person monitors the images on a monitor during the process and optionally makes a change in the process parameters.
- the evaluation or evaluation of the images taken by the at least one camera provides criteria on the basis of which an online control of the freeze-drying process is possible.
- the state of the freeze-dried product can thus be observed at any point in the process, which allows the process parameters to be brought close to the limits of what is physically possible. In this case, it is no longer necessary to resort to limit parameters previously determined in extensive test series while maintaining a safety margin, but the optical online control permits dynamic control or regulation of the freeze-drying process exclusively on the basis of the visually determined instantaneous state of the frozen meat product.
- a method is also preferred in which the images are evaluated by means of an evaluation device.
- the images do not need to be evaluated by a test person, but they are preferably software-supported evaluated by an image processing program and evaluated in terms of the product quality to be guaranteed.
- a method is also preferred in which parameters of the freeze-drying process can be changed by means of the evaluation device. Due to the evaluation of the images delivered by the at least one camera, the parameters of the Freeze-drying process can be adjusted so that a desired product quality is guaranteed.
- a method is preferred in which, based on the evaluation of the images, signals are sent from the evaluation device to a control device of the freeze-drying device, on the basis of which the parameters of the freeze-drying process are changed.
- the images supplied by the at least one camera are thus evaluated by the evaluation device and evaluated in particular with regard to the desired product quality, and signals are sent from the evaluation device to a control device of the freeze-drying device on the basis of this evaluation, which serve to set the parameters of the Freeze drying process to change so that a desired product quality can be maintained.
- the single figure shows schematically the interior 1 of a device for the serial freeze-drying of pharmaceutical solutions in medical hollow bodies.
- three shelves 3, 3 ', 3 " are indicated, which are preferably temperature-controlled, in order to be able to freeze the substances intended for lyophilization in the interior 1 at the start of the freeze-drying process, and to sublimate the solvent during the freeze-drying process
- medical hollow bodies are arranged here as vials 5 are formed. These comprise a substance 7 intended for freeze-drying.
- a camera 9 is provided, which is arranged by way of example on the middle shelf 3 'and can take pictures of at least one of the pharmaceutical solutions or substances 7 intended for freeze-drying.
- only one camera 9 is provided on the middle shelf 3 '. If the process parameters have the same values at each location of the interior 1, it is sufficient, in principle, to observe a vial 5 with a substance 7 by means of the camera 9. However, it is also possible to provide a plurality of cameras 9 which record images of the observed vial 5 and the observed substance 7 from different directions. In this way, it can be ensured that the frozen substance 7 does not thaw, for example, locally on a side which is not observed by a camera 9.
- the process parameters on the various shelves 3, 3 ', 3 typically differ at least somewhat, it may be useful to arrange at least one camera 9 on each of the shelves 3, 3', 3", the images of at least one vial 5 with a substance 7 receives. This ensures that the freeze-drying process is equally controlled on all shelves 3, 3 ', 3 "and can be controlled if necessary. which is under observation by means of a camera 9, are still in an optimal range of values, while they already deviate from the optimum value range on another shelf 3, 3 ', 3 ", so that the desired product quality is not more can be guaranteed.
- the camera 9 can be designed as an analog camera, as a digital camera, as a macro camera, preferably a camera with a macro lens, or as a webcam.
- the images supplied by the at least one camera 9 are electronically recorded and evaluated. This is possible in a particularly simple manner if the camera 9 is a digital camera.
- the camera 9 is miniaturized, so that it has a small space requirement and takes away little space in the interior 1, which is so medical hollow bodies available.
- the camera 9 is preferably triggered at intervals, but can also record images in continuous operation, ie films. However, it is advantageous not to operate the camera 9 in continuous operation, but to have the images recorded at intervals. In this way, the operational heating of the camera 9 clearly leans less, so that the heat emitted by the latter to the interior 1 is minimized.
- the times for taking pictures can be synchronized with relevant process parameters. It can thus be provided that, for example, an increase in pressure in the interior 1 leads to the triggering of at least one camera 9. Of course, other process parameters for timing can be used to capture camera users.
- no illumination device is provided in the interior 1 of a freeze dryer, which allows illumination of the medical hollow body during the process. If the visible part of the electromagnetic spectrum is to be used to record the images by the at least one camera 9, then a lighting device must be arranged in the interior 1, so that sufficient light is available to record the desired images. This lighting device is preferably designed as a cold light source in order to influence the temperature of the interior 1 as little as possible.
- the camera 9 comprises the illumination device.
- the illumination device can be connected to the camera 9 so that it always illuminates exactly the area that the camera 9 picks up. It is particularly advantageous if the illumination device is integrated in the at least one camera 9. Thus, a particularly compact design can be realized.
- the camera 9 in its interior has a higher pressure than the external atmosphere. This could even damage the camera.
- the camera 9 can heat up during its operation.
- the at least one camera 9 is formed thermally insulated.
- the vacuum-tight housing 11, which receives the camera 9, be thermally insulated.
- the at least one camera 9 and / or the at least one vacuum-tight housing 11 rings have particle density.
- the at least one camera 9 and / or the at least one vacuum-tight housing 11 can be sterilized.
- the housing 11 and / or the camera 9 are not arranged on a shelf 3, 3 ', 3 ", but attached directly to a magazine accommodating the medical hollow bodies or vials 5, for example
- the camera 9 or the housing 11 can pass through the entire sterilization and filling or freeze-drying process together with the magazine so that at least one camera 9 or housing 11 can be permanently assigned to one magazine and in principle not
- the data and / or energy transmission from or to the camera 9 takes place wirelessly, so that the magazines can in principle be handled in the same way as if no camera 9 were connected to the magazine
- the camera 9 can, for example, with an antenna for wireless data transmission un d be equipped with a battery for power supply.
- an accumulator can be used.
- an inductive transmission path can be provided which transmits both energy and data from an external source to the camera 9 or in the opposite direction.
- An optical transmission path is also possible.
- a plurality of cameras 9 can be accommodated in one housing 11, but each camera 9 can also be assigned its own housing 11.
- the at least one camera 9 can also be designed as an endoscopic system, which can be introduced, for example, into a vial 5. In this way, the camera 9 can be moved up very close to the substance 7 intended for freeze-drying in order to be able to take up particularly detailed images of the substance 7, for example.
- an endoscopic system can also serve to introduce a light guide via a bushing into the interior 1 of the freeze dryer, through which the images from the interior 1 to an external camera 9 can be forwarded.
- the camera 9 can thus be arranged completely outside the interior 1 and must therefore meet lower requirements for the vacuum tightness, particle density or sterility.
- a plurality of light guides can be distributed in the interior 1, which are led out of the interior 1 via feedthroughs and are optionally assigned to different cameras 9 or a single camera 9. If a single camera 9 is provided, it can be connected to a device which can switch over in time between the image information supplied by the different light guides, so that the camera 9 at different times images from different locations or from different directions in the interior 1 can record.
- Another advantage of such light guides is that they require very little space in the interior 1, so that more space for medical hollow body remains.
- the at least one camera 9 can also be designed such that it uses the invisible region of the electromagnetic spectrum to take pictures. For this she must be sensitive in this area.
- the camera 9 can take thermal images if it is sensitive to the infrared part of the electromagnetic spectrum. This can be advantageous, since on the one hand, a lighting device can be dispensed with, and on the other hand, the product temperature of the substance can be displayed in a spatially resolved manner by false colors. In this way, information complementary to the structure of the substance 7 is obtained by detecting the location-dependent course of the temperature within the substance 7.
- the images taken by the at least one camera 9 of at least one lyophilization-specific pharmaceutical solution or substance 7 should be usable for controlling and / or controlling the freeze-drying process.
- a test person evaluates the images, and optionally adjusts the process parameters such as the temperature, pressure, humidity or the time course of these parameters during the process, or even the total process time to the knowledge gained by the images.
- an evaluation device can be provided which evaluates the images, for example with the aid of an image evaluation program, and in particular assesses them with regard to a desired product quality. On the basis of this evaluation or assessment, it is then possible to make changes to the parameters of the freeze-drying process, which is preferably done automatically.
- the evaluation device may relate on the basis of the evaluation.
- evaluation of the images to send signals to a controller of the freeze-drying device, which are adapted to change the parameters of the freeze-drying process so that a desired product quality is achieved.
- the control device can also take over the timing for taking pictures by the at least one camera 9.
- the recordings can also be triggered by changes in the product parameters.
- a freeze-drying device such as vials 5 are introduced, which contain certain pharmaceutical solutions or substances 7 for freeze-drying.
- At least one camera takes pictures of at least one of the vials 5 or substances 7, which are used to control and / or control the freeze-drying process.
- a test person or an evaluation device which preferably comprises an image evaluation program, can be used.
- the test person or the evaluation device checks the course or progress of the freeze-drying process and optionally intervenes in it by changing process parameters.
- the parameters of the freeze-drying process can then be changed if necessary.
- the parameters of the freeze-drying process may be changed.
Landscapes
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Molecular Biology (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Drying Of Solid Materials (AREA)
Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102008030269A DE102008030269A1 (de) | 2008-06-19 | 2008-06-19 | Vorrichtung zur serienmäßigen Gefriertrocknung |
PCT/EP2009/004312 WO2009153017A2 (de) | 2008-06-19 | 2009-06-16 | Vorrichtung zur serienmässigen gefriertrocknung |
Publications (2)
Publication Number | Publication Date |
---|---|
EP2310781A2 true EP2310781A2 (de) | 2011-04-20 |
EP2310781B1 EP2310781B1 (de) | 2016-08-17 |
Family
ID=41335024
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP09765597.1A Active EP2310781B1 (de) | 2008-06-19 | 2009-06-16 | Vorrichtung und verfahren zur serienmässigen gefriertrocknung |
Country Status (11)
Country | Link |
---|---|
US (1) | US8677649B2 (de) |
EP (1) | EP2310781B1 (de) |
JP (2) | JP5897331B2 (de) |
BR (1) | BRPI0914202B1 (de) |
CA (1) | CA2728365C (de) |
DE (1) | DE102008030269A1 (de) |
ES (1) | ES2595100T3 (de) |
MX (1) | MX2010013372A (de) |
PT (1) | PT2310781T (de) |
RU (1) | RU2494323C2 (de) |
WO (1) | WO2009153017A2 (de) |
Families Citing this family (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102008030269A1 (de) * | 2008-06-19 | 2009-12-24 | Arzneimittel Gmbh Apotheker Vetter & Co. Ravensburg | Vorrichtung zur serienmäßigen Gefriertrocknung |
DK3222952T3 (en) | 2011-09-06 | 2019-04-08 | Rv Holding B V | Method and system for freeze-drying injectable compositions, in particular pharmaceutical compositions |
EP3151662B1 (de) * | 2014-06-09 | 2020-10-21 | Terumo BCT, Inc. | Lyophilisierung |
DE102016100163A1 (de) | 2016-01-05 | 2017-07-06 | Martin Christ Gefriertrocknungsanlagen Gmbh | Gefriertrockner-Steuereinrichtung, Verfahren zum Betrieb derselben, Gefriertrockner und Gefriertrocknungsanlage |
SG11201900479QA (en) | 2016-08-16 | 2019-02-27 | Univ Gent | Method and apparatus and container for freeze-drying |
JP2021529926A (ja) * | 2018-06-29 | 2021-11-04 | ユニバーシテイト ヘント | 製品容量単位の凍結、乾燥および/またはフリーズドライ |
US11243029B2 (en) * | 2019-04-26 | 2022-02-08 | Purdue Research Foundation | Process monitoring and control for lyophilization using a wireless sensor network |
US11054185B1 (en) | 2020-02-24 | 2021-07-06 | Lyophilization Technology, Inc. | Apparatus for lyophilization of products contained in product delivery units |
US20230346641A1 (en) * | 2020-08-20 | 2023-11-02 | Hoffmann-La Roche Inc. | Lyophilisate retainer, method of manufacturing thereof and procedure of drying a substrate |
US20230122361A1 (en) * | 2021-10-20 | 2023-04-20 | DSM Sales & Manufacturing, Inc. | Freeze-drying systems and methods |
Family Cites Families (14)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR1236607A (fr) * | 1959-06-11 | 1960-07-22 | Centre Nat Rech Scient | Procédé et dispositif pour le contrôle et la régulation de la congélation et dudégel de différentes substances, et notamment pour le contrôle et la régulation d'opérations de congélation-dessiccation |
US3627423A (en) * | 1970-02-17 | 1971-12-14 | Schering Corp | Method and apparatus for detecting particular matter in sealed liquids |
SU609037A1 (ru) * | 1972-09-21 | 1978-05-30 | Черновицкий Государственный Медицинский Институт | Устройство дл лиофильной сушки образцов животных и растительных тканей |
DE2854534C3 (de) * | 1978-12-16 | 1982-02-11 | B. Braun Melsungen Ag, 3508 Melsungen | Zahnpulpenfüllmaterial |
JP3212389B2 (ja) * | 1992-10-26 | 2001-09-25 | 株式会社キリンテクノシステム | 固体上の異物検査方法 |
JP3351910B2 (ja) * | 1994-09-01 | 2002-12-03 | エーザイ株式会社 | バイアル瓶の検査方法と装置 |
JP2002014049A (ja) * | 2000-04-13 | 2002-01-18 | Eisai Co Ltd | 凍結乾燥製剤の乾燥前における混入異物の検査方法及びその装置 |
SE0001453D0 (sv) * | 2000-04-19 | 2000-04-19 | Astrazeneca Ab | Method of monitoring a freeze drying process |
DE20214474U1 (de) * | 2002-09-18 | 2004-02-19 | Süverkrüp, Richard, Prof. Dr. | Anlage zum Lyophilisieren von Lösungen, Suspensionen und Dispersionen |
AU2003295867A1 (en) * | 2002-11-21 | 2004-06-18 | Transform Pharmaceuticals, Inc. | Freeze-drying microscope stage apparatus and process of using the same |
JP4474663B2 (ja) * | 2003-08-27 | 2010-06-09 | 努 升島 | ビデオ顕微鏡装置 |
JP2005218686A (ja) * | 2004-02-06 | 2005-08-18 | Shibuya Kogyo Co Ltd | 乾燥滅菌機 |
DE102008030269A1 (de) * | 2008-06-19 | 2009-12-24 | Arzneimittel Gmbh Apotheker Vetter & Co. Ravensburg | Vorrichtung zur serienmäßigen Gefriertrocknung |
JP5661748B2 (ja) * | 2009-05-15 | 2015-01-28 | グラクソスミスクライン・リミテッド・ライアビリティ・カンパニーGlaxoSmithKline LLC | 製造プロセスを制御するための熱画像の利用 |
-
2008
- 2008-06-19 DE DE102008030269A patent/DE102008030269A1/de not_active Ceased
-
2009
- 2009-06-16 US US12/999,021 patent/US8677649B2/en active Active
- 2009-06-16 BR BRPI0914202 patent/BRPI0914202B1/pt active IP Right Grant
- 2009-06-16 JP JP2011513940A patent/JP5897331B2/ja active Active
- 2009-06-16 CA CA2728365A patent/CA2728365C/en active Active
- 2009-06-16 PT PT97655971T patent/PT2310781T/pt unknown
- 2009-06-16 RU RU2011101686/06A patent/RU2494323C2/ru active
- 2009-06-16 WO PCT/EP2009/004312 patent/WO2009153017A2/de active Application Filing
- 2009-06-16 EP EP09765597.1A patent/EP2310781B1/de active Active
- 2009-06-16 MX MX2010013372A patent/MX2010013372A/es active IP Right Grant
- 2009-06-16 ES ES09765597.1T patent/ES2595100T3/es active Active
-
2014
- 2014-08-08 JP JP2014162805A patent/JP6062402B2/ja active Active
Non-Patent Citations (1)
Title |
---|
See references of WO2009153017A3 * |
Also Published As
Publication number | Publication date |
---|---|
RU2494323C2 (ru) | 2013-09-27 |
BRPI0914202A2 (pt) | 2015-11-03 |
BRPI0914202B1 (pt) | 2019-12-03 |
JP2014224677A (ja) | 2014-12-04 |
PT2310781T (pt) | 2016-11-08 |
ES2595100T3 (es) | 2016-12-27 |
CA2728365C (en) | 2016-03-22 |
JP5897331B2 (ja) | 2016-03-30 |
DE102008030269A1 (de) | 2009-12-24 |
JP2011524512A (ja) | 2011-09-01 |
RU2011101686A (ru) | 2012-07-27 |
WO2009153017A3 (de) | 2010-10-14 |
CA2728365A1 (en) | 2009-12-23 |
MX2010013372A (es) | 2011-03-21 |
EP2310781B1 (de) | 2016-08-17 |
JP6062402B2 (ja) | 2017-01-18 |
WO2009153017A2 (de) | 2009-12-23 |
US20110099836A1 (en) | 2011-05-05 |
US8677649B2 (en) | 2014-03-25 |
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